WO2020042208A1 - 一种耐高低温近红外吸收滤光片及其制备方法 - Google Patents

一种耐高低温近红外吸收滤光片及其制备方法 Download PDF

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WO2020042208A1
WO2020042208A1 PCT/CN2018/104311 CN2018104311W WO2020042208A1 WO 2020042208 A1 WO2020042208 A1 WO 2020042208A1 CN 2018104311 W CN2018104311 W CN 2018104311W WO 2020042208 A1 WO2020042208 A1 WO 2020042208A1
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parts
mass
hours
temperature resistant
optical polymer
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王丽熙
张其土
管永康
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苏州讯能光电科技有限公司
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/22—Absorbing filters
    • G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C08L33/10—Homopolymers or copolymers of methacrylic acid esters
    • C08L33/12—Homopolymers or copolymers of methyl methacrylate
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics

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  • the invention belongs to the field of night vision compatible materials, and relates to a high and low temperature resistant near-infrared absorption filter and a preparation method thereof.
  • Night vision compatible materials need to have good cut-off performance for the 660nm ⁇ 930nm red light region and near-infrared red light region, while ensuring sufficient transmittance in the visible light region of 400nm ⁇ 630nm.
  • the material needs to have excellent resistance to high and low temperatures.
  • Traditional night vision compatible materials such as colored glass materials, plastic-glass laminated composites, etc. have the disadvantages of complicated processes, high prices and high quality.
  • Chinese patent document CN102031047A discloses a "night vision-compatible near-infrared absorbing film material and a preparation method thereof". Although the process is simple and the material quality is light, the material is easily deformed in high and low temperature environments and does not have good environmental stability. . Therefore, it is necessary to prepare a near-infrared absorbing material resistant to high and low temperature environments.
  • the present invention provides a good cut-off performance in the red light region of 660 nm to 930 nm and the near-infrared red light region, while ensuring sufficient transmittance in the visible light region of 400 nm to 630 nm, and can Near-infrared absorption filter material used under low temperature environment for a long time and preparation method thereof.
  • the present invention discloses a high and low temperature resistant near-infrared absorber filter.
  • the components and parts by weight are as follows: 0.2 to 0.5 parts by mass of near-infrared absorber and 30 to 50 parts by mass of organic solvent. , 80-100 parts by mass of optical polymer pellets;
  • the near-infrared absorbing agent is a thiodiene-type nickel complex dye or an o-phenylenediamine-type complex dye.
  • the optical polymer pellets are polymethyl methacrylate.
  • the organic solvent is chloroform, toluene or acetone.
  • the method for preparing the high and low temperature resistant near-infrared absorption filter is as follows:
  • optical polymer pellets are sealed and dried at 85 ° C for 4 hours;
  • the near-infrared absorbing material prepared by the present invention has excellent high temperature resistance and low temperature performance.
  • the obtained filter has good cut-off performance for light in a wavelength range of 650-900 nm, and has good transmittance in the visible light region.
  • FIG. 1 is a transmission spectrum of a filter material according to the present invention.
  • Figure 2 shows the transmission curve of the filter material before and after the low temperature experiment.
  • Figure 3 shows the transmission curve of the filter material before and after the high temperature experiment.
  • optical polymer pellets polymethyl methacrylate are sealed and dried at 85 ° C for 4 hours;
  • optical polymer pellets polymethyl methacrylate are sealed and dried at 85 ° C for 4 hours;
  • optical polymer pellets polymethyl methacrylate are sealed and dried at 85 ° C for 4 hours;
  • optical polymer pellets polymethyl methacrylate are sealed and dried at 85 ° C for 4 hours;
  • optical polymer pellets polymethyl methacrylate are sealed and dried at 85 ° C for 4 hours;

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Optical Filters (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

一种耐高低温近红外吸收滤光片及其制备方法，制备方法为取近红外吸收剂0.2～0.5质量份添加到30～50质量份有机溶剂中，搅拌均匀后，将80～100质量份光学聚合物粒料加入溶液中并搅拌，得到近红外吸收涂层材料。近红外吸收材料具有优秀的耐高温、低温性能。滤光片对波段为650～900nm范围内光线具有良好截止性能，并在可见光区域具有较好透过率。

Description

一种耐高低温近红外吸收滤光片及其制备方法 技术领域
本发明属于夜视兼容材料领域，本发明涉及一种耐高低温近红外吸收滤光片及其制备方法。
背景技术
夜视兼容材料需对660nm～930nm红光区及近红外红光区有良好的截止性能，同时保证在400nm～630nm可见光区有足够的透过率。此外，该材料还需具有优秀的耐高低温性能。传统的夜视兼容材料如有色玻璃材料、塑料-玻璃层压复合材料等具有工艺复杂、价格昂贵且质量大等缺点。而中国专利文献CN102031047A公开了一种“夜视兼容近红外吸收膜材料及其制备方法”，虽然其工艺简单，材料质量轻，但是在高低温环境下材料容易变形，不具有良好的环境稳定性。因此，制备一种耐高低温环境的近红外吸收材料是非常必要的。
发明内容
要解决的技术问题：本发明提供了一种在660nm～930nm红光区及近红外红光区有良好的截止性能，同时保证在400nm～630nm可见光区有足够的透过率，并且能在高低温环境下长期使用的近红外吸收滤光片材料及其制备方法。
技术方案：为了解决上述问题，本发明公开了一种耐高低温近红外吸收剂滤光片，各组分及重量份如下：近红外吸收剂0.2～0.5质量份，有机溶剂30～50质量份，光学聚合物粒料80～100质量份；
优选的，所述的近红外吸收剂为硫代双烯型镍络合染料或邻苯二胺型络合染料。
优选的，所述的光学聚合物粒料为聚甲基丙烯酸甲酯。
优选的，所述有机溶剂为氯仿、甲苯或丙酮。
所述的一种耐高低温近红外吸收滤光片的制备方法，步骤如下：
(1)将光学聚合物粒料于85℃下密封干燥4小时；
(2)按质量百分比称取光吸收剂和光学聚合物粒料；
(3)按比例称取氯仿、甲苯或丙酮，将光吸收剂和光学聚合物粒料溶解其中，搅拌1～2小时，设定转速为200r/min～300r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化4～6小时。
有益效果：本发明制备的近红外吸收材料具有优秀的耐高温、低温性能。所得滤光片对波段为650～900nm范围内光线具有良好截止性能，并在可见光区域具有较好透过率。
附图说明
图1为本发明滤光材料的透射光谱。
图2为低温实验前后滤光材料透射曲线。
图3为高温实验前后滤光材料透射曲线。
具体实施方式
实施例1
(1)将光学聚合物粒料聚甲基丙烯酸甲酯于85℃下密封干燥4小时；
(2)称取近红外吸收剂硫代双烯型镍络合染料0.2质量份和聚甲基丙烯酸甲酯80质量份；
(3)称取氯仿30质量份，将近红外吸收剂和光学聚合物粒料溶解其 中，搅拌1小时，设定转速为300r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化4小时。
实施例2
(1)将光学聚合物粒料聚甲基丙烯酸甲酯于85℃下密封干燥4小时；
(2)称取近红外吸收剂邻苯二胺型络合染料0.5质量份和聚甲基丙烯酸甲酯100质量份；
(3)按比例称取甲苯50质量份，将近红外吸收剂和光学聚合物粒料溶解其中，搅拌2小时，设定转速为200r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化6小时。
实施例3
(1)将光学聚合物粒料聚甲基丙烯酸甲酯于85℃下密封干燥4小时；
(2)称取近红外吸收剂硫代双烯型镍络合染料0.2质量份和聚甲基丙烯酸甲酯100质量份；
(3)称取丙酮30份，将近红外吸收剂和光学聚合物粒料溶解其中，搅拌1小时，设定转速为200r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化4小时。
实施例4
(1)将光学聚合物粒料聚甲基丙烯酸甲酯于85℃下密封干燥4小时；
(2)称取近红外吸收剂邻苯二胺型络合染料0.5质量份和聚甲基丙烯 酸甲酯80质量份；
(3)称取丙酮40份，将近红外吸收剂和光学聚合物粒料溶解其中，搅拌1小时，设定转速为250r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化6小时。
实施例5
(1)将光学聚合物粒料聚甲基丙烯酸甲酯于85℃下密封干燥4小时；
(2)称取近红外吸收剂硫代双烯型镍络合染料0.3质量份和聚甲基丙烯酸甲酯90质量份；
(3)称取氯仿50份，将近红外吸收剂和光学聚合物粒料溶解其中，搅拌1小时，设定转速为300r/min；
(4)置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化5小时。

Claims (5)

  1. 一种耐高低温近红外吸收剂滤光片，其特征在于各组分及重量份如下：近红外吸收剂0.2～0.5质量份，有机溶剂30～50质量份，光学聚合物粒料80～100质量份。
  2. 根据权利要求1所述的一种耐高低温近红外吸收滤光片，其特征在于，所述的近红外吸收剂为硫代双烯型镍络合染料或邻苯二胺型络合染料。
  3. 根据权利要求1所述的一种耐高低温近红外吸收滤光片，其特征在于，所述的光学聚合物粒料为聚甲基丙烯酸甲酯。
  4. 根据权利要求1所述的一种耐高低温近红外吸收滤光片，其特征在于，所述有机溶剂为氯仿、甲苯或丙酮。
  5. 根据权利要求1所述的一种耐高低温近红外吸收滤光片的制备方法，其特征在于，所述的制备方法步骤如下：
    步骤一，将光学聚合物粒料于85℃下密封干燥4小时；
    步骤二，按质量百分比称取近红外吸收剂和光学聚合物粒料；
    步骤三，按比例称取氯仿、甲苯或丙酮，将光吸收剂和光学聚合物粒料溶解其中，搅拌1～2小时，设定转速为200r/min～300r/min；
    步骤四，置于比色皿中静置24小时，待溶剂完全挥发后转移至80℃烘箱中固化4～6小时。
PCT/CN2018/104311 2018-08-31 2018-09-06 一种耐高低温近红外吸收滤光片及其制备方法 WO2020042208A1 (zh)

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CN113715286A (zh) * 2020-12-24 2021-11-30 杏晖光学（厦门）有限公司 一种军工用激光防护镜片的制备工艺

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CN110646950A (zh) * 2019-09-10 2020-01-03 江苏淘镜有限公司 一种带防近红外线ira功能的镜片及其制造工艺
CN111562641B (zh) * 2020-05-25 2022-04-29 南京邮电大学 一种夜视兼容红外滤光片及其制备方法
CN112684531B (zh) * 2020-12-29 2022-07-26 上海戎科特种装备有限公司 一种耐高低温且可见光高透过的夜视兼容滤光片及制备方法
CN113138437A (zh) * 2021-03-08 2021-07-20 长春理工大学 一种宽带近红外吸收滤光片及其制备方法

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